CN103820253B - Technique and the device of powdery MES particle is prepared in a kind of serialization - Google Patents
Technique and the device of powdery MES particle is prepared in a kind of serialization Download PDFInfo
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- CN103820253B CN103820253B CN201410048579.9A CN201410048579A CN103820253B CN 103820253 B CN103820253 B CN 103820253B CN 201410048579 A CN201410048579 A CN 201410048579A CN 103820253 B CN103820253 B CN 103820253B
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- 239000002245 particle Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 42
- 238000007701 flash-distillation Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 23
- 150000002148 esters Chemical class 0.000 claims abstract description 22
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 20
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000008187 granular material Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 20
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 14
- 238000006386 neutralization reaction Methods 0.000 claims description 14
- 230000007246 mechanism Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 150000001447 alkali salts Chemical class 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000006277 sulfonation reaction Methods 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000002801 charged material Substances 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 description 19
- 238000004090 dissolution Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000005453 pelletization Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005550 wet granulation Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010410 dusting Methods 0.000 description 2
- -1 fatty acids methyl ester Chemical class 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 229940023462 paste product Drugs 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 229960003010 sodium sulfate Drugs 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 229940038773 trisodium citrate Drugs 0.000 description 2
- 206010009866 Cold sweat Diseases 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 229920003109 sodium starch glycolate Polymers 0.000 description 1
- 229940079832 sodium starch glycolate Drugs 0.000 description 1
- 239000008109 sodium starch glycolate Substances 0.000 description 1
- 229940056729 sodium sulfate anhydrous Drugs 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 235000019263 trisodium citrate Nutrition 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Landscapes
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to technique and device that powdery MES particle is prepared in a kind of serialization. The technical process provided that object is to provide is simple; The preparation facilities structure provided is simple. Technical scheme is: the technique of powdery MES particle is prepared in a kind of serialization, comprises the following steps: 1) pulverulent mixture of neutralizing agent, coating agent, stablizer and fatty acid methyl ester acid esters enter a high-shear reactor by a certain percentage; 2) flash distillation dryer is entered after forming MES particle; 3) the MES particle making to obtain maintains certain granules degree; 4) mixed airflow exporting out from flash distillation dryer enters cyclonic separator and is separated; 5) finished product is obtained. A kind of powdery MES particle serialization preparation facilities, this device comprises the high-shear reactor, flash distillation dryer, cyclone separator, sack cleaner and the induced draft fan that are connected successively; High-shear reactor is shaped with acid esters entrance, powder body entrance, gas inlet respectively and connects the material outlet of flash distillation dryer.
Description
Technical field
The present invention relates to the manufacturing process of a kind of surfactant particles, especially the manufacturing process of methyl sodiosul foaliphatate particle.
Background technology
Methyl sodiosul foaliphatate (MES) is a kind of novel anion surfactant, excellent property, has a extensive future, and petroleum base tensio-active agent can be replaced such as LAS, AOS etc., meet the overall development trend of resource and environment. Research shows, methyl sodiosul foaliphatate has excellent soil removability, and skin irritation is little, and performance is gentle, without irritated, toxicity is low, security height, can in a large number in various liquid, powdered detergent.
The production main processes of MES is the lipid acid obtained through techniques such as hydrolysis or saponification acidolysis by natural animal-plant oil, fatty acid methyl ester is obtained again with methanol esterification, methyl esters and gas phase sulfur trioxide sulfonation, resterification, decolouring, neutralization obtain paste product, or continuation drying obtains powder-like product. Wherein paste product content is about 30%, and its product because the reduction of the envrionment temperature such as storage and isolate water-yielding stratum and similar bean dregs sample solidification layer, can cause material uneven, affect outward appearance and use; 80% powdery or chip solid MES are producing in drying process, and material can experience by lotion, high viscosity fluid, and the phase change of the three phases of most Zhongdao chip solid or powder body, exists energy consumption big, the problem of continuous production difference.
The application of current MES in washing powder remains in certain restriction, this is mainly owing to the production of current laundry powder mainly adopts high tower spraying (high-temperature hot-air in 250��350 DEG C is produced), owing to temperature of dusting is higher, and powder spraying slurry is generally in alkalescence, easily causes the decomposition of MES in process of dusting.
For addressing this problem, after generally tending to now, join technique, namely first MES is processed into MES particle and is fitted on afterwards again in washing powder. The production of granular MES product, currently mainly it is divided into wet granulation and non-slurry pelletizing, wherein wet granulation is to receive CN103320235A disclosed in Ace " particle of a kind of fatty acids methyl ester sulfonate and its preparation method " as representative, it adopts paste MES(and 30%MES) carry out wet granulation with zeolite, silicate, modified starch and wilkinite, then drying, sub-sieve obtain; Wherein non-slurry pelletizing is taking CN102277238A disclosed in enlightening health biology as representative; it adopts 80% sheet MES to be raw material; after mixing with Sodium sulfate anhydrous.min(99), 4A zeolite, sodium starch glycolate and wilkinite; the extruding pelletization when there is outside protection wind, is cooled to hardening completely through-5��30 DEG C of dry airs and obtains particle. These preparation technologies all have its weak point:
1) adopting wet granulation, moisture higher in particle, it is necessary to dry further, energy consumption is relatively big, and in drying process, temperature control is too high also there will be the phenomenons such as particle is clamminess; Adopt non-slurry pelletizing, it is necessary to selecting the MES of high-content, high-content MES have passed through the drying process of highly energy-consuming in making.
2) Krafft's point due to MES self is higher, and the dissolution in low temperature causing these two kinds of MES particles is poor.
3) technique process is complicated, and production efficiency is lower, and production capacity is subject to bigger restriction.
Therefore, how to develop that a kind of technique is simple, energy-conserving and environment-protective, powdery MES product that production efficiency high and low temperature solvability is good preparation method, MES is applied in washing powder, is a difficult problem urgently to be resolved hurrily.
Summary of the invention
It is an object of the invention to the deficiency overcome in above-mentioned background technology, it is provided that technique and the preparation facilities thereof of powdery MES particle is prepared in a kind of serialization. The technique provided has that technical process is simple, energy-conserving and environment-protective, feature that production efficiency is high, the powdery MES particle flow obtained is good, not easily bond, and dissolution in low temperature is good, joins technique after can being directly used in washing powder; The preparation facilities structure provided is simple, easy to manufacture, and cost is lower.
The technical scheme of the present invention is:
A technique for powdery MES particle is prepared in serialization, comprises the following steps
1) pulverulent mixture of neutralizing agent, coating agent, stablizer enters a high-shear reactor by a certain percentage, and the fatty acid methyl ester acid esters that fatty acid methyl ester is formed after sulfonation simultaneously also enters high-shear reactor by a certain percentage;
2) material stops 10��60s in high-shear reactor reactor, neutralization reaction occurs and is wrapped to form MES particle; Then opening induced draft fan, MES particle enters flash distillation dryer after being exported from high-shear reactor by the dual function that centrifugal force and wind send;
3) after the MES particle of flash distillation dryer process is exported from flash distillation dryer top by upstream effect, cyclonic separator is entered, period utilizes air-flow to remove neutralization heat and a small amount of water of neutralization generation, makes MES particle cooling (be cooled to and be less than 40 DEG C) and dry (be dried to water content and be less than 5%); Make the thicker MES particle of part return to high-shear reactor resume with control blast to pulverize further so that the MES particle arrived maintains certain granules degree;
4) mixed airflow exporting out from flash distillation dryer enters cyclonic separator and is separated, and the pulverulent material isolated directly enters finished powder storehouse, after the mixed airflow isolated enters sack cleaner dedusting, emptying by induced draft fan;
5) in finished powder storehouse, namely MES particle packaging obtains finished product; The part dust that bag-type dust separation obtains returns to high-shear reactor entrance and continues reaction granulation;
Charged material weight ratio in described step 1) is: fatty acid methyl ester acid esters 20��40 parts, neutralizing agent 2��10 parts, coating agent 50��75 parts, stablizer 0��1 part.
Described neutralizing agent is the mixing of one or two or more kinds arbitrary proportion in basic salt, basic oxide, alkaline hydrated oxide; Its metal ion is at least one in sodium, potassium, magnesium, calcium. Described basic salt is the mixture of one or two or more kinds arbitrary proportion in carbonate, supercarbonate, silicate, described basic oxide are the mixing of one or two or more kinds arbitrary proportion in sodium oxide, potassium oxide, magnesium oxide, calcium oxide, and described alkaline hydrated oxide is mixing that are a kind of in sodium hydroxide, potassium hydroxide or two kinds of arbitrary proportions.
Described coating agent is the mixing of one or two or more kinds arbitrary proportion in 4A zeolite, wilkinite, diatomite, sodium sulfate.
Described stablizer is the mixing of one or two or more kinds arbitrary proportion in citric acid, Citrate trianion, phosphoric acid, phosphoric acid salt, hydrophosphate, metal ion wherein be receive, at least one in potassium, magnesium calcium.
In the pulverulent mixture of described neutralizing agent, coating agent, stablizer, it is also possible to adding portion discoloring agent, tinting material; Described discoloring agent can be hypochlorite, percarbonate etc., metal ion wherein be receive, at least one in potassium, magnesium calcium.
A kind of powdery MES particle serialization preparation facilities, it is characterised in that this device comprises the high-shear reactor, flash distillation dryer, cyclone separator, sack cleaner and the induced draft fan that are connected successively by pipeline; The horizontal layout of described high-shear reactor and be shaped with respectively acid esters entrance, powder body entrance, gas inlet and connect flash distillation dryer material outlet.
Described high-shear reactor comprises: a horizontal layout and the cylindrical reactor vessel, being shaped with acid esters entrance, powder body entrance, material outlet and gas inlet respectively are positioned in reaction vessel and material in reaction vessel carry out the stirring cutting mechanism of high speed shear and drives the transmission rig stirring cutting mechanism; Described acid esters entrance, powder body entrance are positioned at one end of reactor; Gas inlet, material outlet are positioned at the other end of reactor.
Described stirring cutting mechanism comprises and passes through reaction vessel two ends and the stir shaft coaxially arranged with reaction vessel, be positioned at reaction vessel and be distributed on multiple agitating vane of stir shaft circumferential surface and be fixed on some baffle plates of reaction vessel inwall.
One end of described agitating vane is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane also line around its two ends tilt certain angle, to form the drive surface promoting material to move along reaction vessel axis.
Described baffle plate is the ring plate being arranged between adjacent two baffle plates, the circumferential periphery of this flat board is along being fixed on reaction vessel inwall, and inner periphery edge stretches toward reaction vessel internal diameter direction and keeps with described stir shaft certain spacing as the passage of Flow of Goods and Materials.
The shell of described flash distillation dryer is a cylinder vertically installed, and mixed gas outlet is positioned at cylinder top, and material inlet is positioned at cylinder bottom and directly communicates with the material outlet of high speed shear device.
Described cyclone separator comprises cyclonic separator and is positioned at the finished powder storehouse below cyclonic separator; Described cyclonic separator opening for feed is exported by the mixed airflow of pipeline communication flash distillation dryer; Described cyclonic separator is one or more than two and is connected in series into.
The present invention compared with prior art, has following outstanding advantage:
1) the direct Neutralizing titers of fatty acid methyl ester acid esters is used, the MES particle moisture content less obtained (< 3%), simple drying just can obtain qualified product, avoids and uses in high tower spray drying, and energy consumption high material easily decomposes.
2) neutralization parcel completes simultaneously, the MES particle component that obtains evenly, avoid in conventional granulation process the shortcomings such as coating agent easily departs from, particle component is uneven existed; Simultaneously due to coating agent etc. fabulous be scattered in MES, can there is more microbubble in finished product MES particle when particularly using carbonate to make neutralizing agent, can greatly improve the dissolution in low temperature of MES particle.
3) directly utilizing neutralization heat, be dried by MES particle, capacity usage ratio height (compares with CN103320235A, CN102277238A, can save energy more than 70%);
4) in conjunction with high-shear reactor and flash distillation dryer, the material particles degree obtained is evenly controlled, and particle diameter is at 30��50 orders, it is not necessary to pulverize further.
5) realizing the continuous prodution of granulation, production efficiency improves (comparing with CN102277238A, production efficiency improves 500%) greatly.
6) apparatus structure is simple, and it is easily convenient to manufacture, and cost is lower.
Accompanying drawing explanation
Fig. 1 is the structural representation of powdery MES particle serialization preparation facilities;
Fig. 2 is the structural representation of high-shear reactor in Fig. 1 device.
Wherein 1 is fatty acid methyl ester acid esters, 2 is the mixture of neutralizing agent, coating agent and stablizer, and 3 is air, and 4 is high-shear reactor, 5 is flash distillation dryer, 6 is cyclone separator, and 7 is product outlet, and 8 is sack cleaner, 9 is dust outlet, 10 is induced draft fan, and 11 is input funnel, 6-1 finished powder storehouse;
1-1 is powder body entrance, and 1-2 is acid esters entrance, and 1-3 is gas inlet, and 1-4 is material outlet, and 1-5 is agitating vane, and 1-6 is baffle plate, and 1-7 is shear agitation mechanism, and 1-8 is cylindrical reactor vessel, and 1-9 is transmission rig, and 1-10 is stir shaft.
Embodiment
Below in conjunction with accompanying drawing, invention is described further.
The thinking of the present invention utilizes fatty acid methyl ester acid esters directly and neutralizing agent, coating agent and stablizer direct Neutralizing titers in high-shear reactor, and utilize normal temperature wind to move and go neutralization heat and the dry de-a small amount of water produced except reaction, optionally make big footpath particle continue to return to high-shear reactor with control wind pressure and wind speed and do to pulverize further. Here high-shear reactor is reaction granulating equipment, can play again porphyrization further. This avoid in conventional MES granulation, the shortcomings such as the dry energy consumption height that brings, equipment are complicated, and equipment is simple, utilization ratio height, it is possible to realize continuous and stable production, drastically increases production efficiency. Simultaneously owing to neutralization parcel completes simultaneously, the MES particle component that obtains evenly, avoid in conventional granulation process the shortcomings such as coating agent easily departs from, particle component is uneven existed, coating agent etc. are evenly distributed in MES particle simultaneously; Neutralizing agent adopts basic salt (preferably use carbonate, supercarbonate, or use silicate), basic oxide (mixing of one or two or more kinds arbitrary proportion in preferential oxidation sodium, potassium oxide, magnesium oxide, calcium oxide), alkaline hydrated oxide (mixing of a kind of or two kinds of arbitrary proportions in preferred sodium hydroxide, potassium hydroxide); Producing containing more Minute pores in the MES particle obtained, these can greatly improve the dissolution in low temperature of MES particle. The effect of stablizer makes the pH value of neutralization process more stable, prevents the decomposition that peracid is crossed alkali factor and caused product.
As seen from the figure, device of the present invention is formed primarily of high-shear reactor 4, flash distillation dryer 5, cyclone separator 6, sack cleaner 8 and induced draft fan 10. Wherein the main effect of high-shear reactor makes MES acid esters and neutralizing agent, the rapid contact reacts of coating agent shear granulation, Large stone particle is realized further pulverizing simultaneously; The main effect of flash distillation dryer utilizes normal temperature wind to be lowered the temperature by MES particle and take off and be dried except a small amount of water; MES particle is collected in the main effect of cyclone separator.
In described high-shear reactor: the horizontal layout of cylindrical reactor vessel 1-8, the mixed powder that left end is shaped with fatty acid methyl ester acid esters entrance 1-2 and powder body entrance 1-1(neutralizing agent, coating agent and stablizer respectively can directly transport to this powder body entrance, or transport to this powder body entrance by input funnel 11), right-hand member is shaped with material outlet 1-4, gas inlet 1-3; It is positioned at reaction vessel, the motor-driven belt wheel mechanism of transmission rig 1-9(for material in reaction vessel being carried out the shear agitation mechanism 1-7 of shear agitation) then shear agitation mechanism is driven. In shear agitation mechanism, stir shaft 1-10 axially passes through reaction vessel, and coaxially arranged with reaction vessel; The part stir shaft circumferential surface being positioned at reaction vessel, is uniformly fixed wtih multiple agitating vane 1-5, and some baffle plate 1-6 are fixed on reaction vessel inwall (baffle number is determined as required, shows 2 baffle plates in figure).
One end that above-mentioned agitating vane (is generally plane) is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane also line around its two ends tilt certain angle (angle formed between plane that namely agitating vane tilts and stir shaft cross section), to form the drive surface that promotion material moves along reaction vessel axis. The size of described angle determines the speed that material moves, and can be 0-30 degree usually; Specifically determine as required.
Described baffle plate is the ring plate being arranged between adjacent two baffle plates; This flat board is also coaxially arranged with reaction vessel, its circumferential periphery is along being fixed on reaction vessel inwall, inner periphery edge stretches toward reaction vessel internal diameter direction and keeps certain spacing (spacing size sets as required) with described stir shaft, forms the passage of Flow of Goods and Materials.
Above-mentioned high-shear reactor can simply be processed and obtain, and above-mentioned flash distillation dryer, cyclone separator, sack cleaner and induced draft fan can all obtain in outsourcing.
Illustrate further below by way of specific embodiment.
Embodiment 1
1,1t/hMES particle production line
Sodium carbonate, 4A zeolite, citric acid (weight ratio 7:9:1) are with the flow of 700kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 300kg/h, carry out Neutralizing titers wherein; High-shear reactor selects the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 55 DEG C; Material exports and enters flash distillation dryer more afterwards, and unlatching induced draft fan makes material in flash distillation dryer lower the temperature rapidly and take off to remove to neutralize and produces moisture simultaneously; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtained is as follows:
| Index | Result |
| Actives, % | 30.6 |
| Disodium salt (folding hundred), % | 3.4 |
| Tap density, g/ml | 0.66 |
| Granularity D90, ��m | 380 |
| Dissolution in low temperature | Qualified |
2,1t/hMES particle production line
Sodium bicarbonate, sodium sulfate and Trisodium Citrate (weight ratio 2:5:1) are with the flow of 650kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 350kg/h, carry out Neutralizing titers wherein; High-shear reactor selects the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 57 DEG C; Material exports and enters flash distillation dryer more afterwards, and unlatching induced draft fan makes material in flash distillation dryer lower the temperature rapidly and take off to remove to neutralize and produces moisture simultaneously; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtained is as follows:
| Index | Result |
| Actives, % | 35.1 |
| Disodium salt (folding hundred), % | 2.7 |
| Tap density, g/ml | 0.71 |
| Granularity D90, ��m | 371 |
| Dissolution in low temperature | Qualified |
3,1t/hMES particle production line
Sodium carbonate, wilkinite and sodium phosphate (weight ratio 7:9:1) are with the flow of 700kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 300kg/h, carry out Neutralizing titers wherein; High-shear reactor selects the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 55 DEG C; Material exports and enters flash distillation dryer more afterwards, and unlatching induced draft fan makes material in flash distillation dryer lower the temperature rapidly and take off to remove to neutralize and produces moisture simultaneously; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtained is as follows:
| Index | Result |
| Actives, % | 30.6 |
| Disodium salt (folding hundred), % | 2.6 |
| Tap density, g/ml | 0.69 |
| Granularity D90, ��m | 371 |
| Dissolution in low temperature | Qualified |
4,1t/hMES particle production line
Sodium carbonate, 4A zeolite and Trisodium Citrate (weight ratio 1:20:0.05) are with the flow of 800kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 200kg/h, carry out Neutralizing titers wherein; High-shear reactor selects the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 51 DEG C; Material exports and enters flash distillation dryer more afterwards, and unlatching induced draft fan makes material in flash distillation dryer lower the temperature rapidly and take off to remove to neutralize and produces moisture simultaneously; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtained is as follows:
| Index | Result |
| Actives, % | 21.6 |
| Disodium salt (folding hundred), % | 2.6 |
| Tap density, g/ml | 0.64 |
| Granularity D90, ��m | 367 |
| Dissolution in low temperature | Qualified |
Claims (7)
1. a method for powdery methyl sodiosul foaliphatate particle is prepared in serialization, comprises the following steps
1) pulverulent mixture of neutralizing agent, coating agent, stablizer enters a high-shear reactor by a certain percentage, and simultaneously the fatty acid methyl ester acid esters of fatty acid methyl ester after sulfonation also enters high-shear reactor by a certain percentage;
2) material stops 10��60s in high-shear reactor reactor, neutralization reaction occurs and is wrapped to form methyl sodiosul foaliphatate particle; Then flash distillation dryer is entered after exporting from high-shear reactor;
3) after the methyl sodiosul foaliphatate particle of flash distillation dryer process exports, enter cyclonic separator, carry out cooling and drying; Make simultaneously part relatively crude fatty acid methyl ester sodium sulfonate particle return to high-shear reactor resume and pulverize further, make the methyl sodiosul foaliphatate particle of acquisition maintain certain granules degree;
4) mixed airflow exporting out from flash distillation dryer enters cyclonic separator and is separated, and the pulverulent material isolated directly enters finished powder storehouse, and the mixed airflow isolated is emptying after entering sack cleaner dedusting;
5) in finished powder storehouse, namely methyl sodiosul foaliphatate particle packaging obtains finished product; The part dust that bag-type dust separation obtains returns to high-shear reactor entrance and continues reaction granulation;
Described step 1) in charged material weight ratio be: fatty acid methyl ester acid esters 20��40 parts, neutralizing agent 2��10 parts, coating agent 50��75 parts, stablizer 0��1 part;
Described neutralizing agent is the mixing of one or two or more kinds arbitrary proportion in basic salt, basic oxide, alkaline hydrated oxide; Metal ion wherein is at least one in sodium, potassium, magnesium, calcium;
Described coating agent is the mixing of one or two or more kinds arbitrary proportion in 4A zeolite, wilkinite, diatomite, sodium sulfate;
Described stablizer is the mixing of one or two or more kinds arbitrary proportion in citric acid, Citrate trianion, phosphoric acid, phosphoric acid salt, hydrophosphate; Metal ion wherein is at least one in sodium, potassium, magnesium, calcium.
2. a powdery methyl sodiosul foaliphatate particle serialization preparation facilities, it is characterised in that this device comprises the high-shear reactor (4), flash distillation dryer (5), cyclone separator (8), sack cleaner and the induced draft fan that are connected successively by pipeline; The horizontal layout of described high-shear reactor and be shaped with respectively acid esters entrance (1-2), powder body entrance (1-1), gas inlet (1-3) and connect flash distillation dryer material outlet (1-4).
3. powdery methyl sodiosul foaliphatate particle serialization preparation facilities according to claim 2, it is characterised in that: described high-shear reactor comprises: a horizontal layout and the cylindrical reactor vessel, being shaped with fatty acid methyl ester acid esters entrance, powder body entrance, material outlet and gas inlet respectively are positioned in reaction vessel and material in reaction vessel carry out the stirring cutting mechanism of high speed shear and drives the transmission rig stirring cutting mechanism; Described fatty acid methyl ester acid esters entrance, powder body entrance are positioned at one end of reactor; Gas inlet, material outlet are positioned at the other end of reactor.
4. powdery methyl sodiosul foaliphatate particle serialization preparation facilities according to claim 3, it is characterised in that: described stirring cutting mechanism comprises and passes through reaction vessel two ends and the stir shaft (1-10) coaxially arranged with reaction vessel, be positioned at reaction vessel and be distributed on multiple agitating vanes (1-5) of stir shaft circumferential surface and be fixed on some the baffle plates (1-6) of reaction vessel inwall.
5. powdery methyl sodiosul foaliphatate particle serialization preparation facilities according to claim 4, it is characterised in that: one end of described agitating vane is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane also line around its two ends tilt certain angle, to form the drive surface promoting material to move along reaction vessel axis.
6. powdery methyl sodiosul foaliphatate particle serialization preparation facilities according to claim 5, it is characterized in that: described baffle plate is the ring plate being arranged between adjacent two baffle plates, the circumferential periphery of this flat board is along being fixed on reaction vessel inwall, and inner periphery edge stretches toward reaction vessel internal diameter direction and keeps with described stir shaft certain spacing as the passage of Flow of Goods and Materials.
7. powdery methyl sodiosul foaliphatate particle serialization preparation facilities according to claim 6, it is characterised in that: described cyclone separator comprises cyclonic separator and is positioned at the finished powder storehouse below cyclonic separator; Described cyclonic separator opening for feed is exported by the mixed airflow of pipeline communication flash distillation dryer; Described cyclonic separator is one or more than two and is connected in series into.
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| CN105254540B (en) * | 2015-10-30 | 2017-03-22 | 嘉兴赞宇科技有限公司 | Preparation method and device for powdery fatty acid methyl ester sodium sulfonate |
| CN107033047B (en) * | 2017-05-09 | 2019-03-26 | 濮阳宏业环保新材料股份有限公司 | A kind of stabilizer improving thiourea dioxide hydrothermal stability |
| CN107159064A (en) * | 2017-05-19 | 2017-09-15 | 江苏和福特种气体有限公司 | A kind of horizontal gas solid reactor |
| CN108727233B (en) * | 2018-07-27 | 2024-02-27 | 赞宇科技集团股份有限公司 | Dry forming process and device for improving low-temperature solubility of alpha-sodium methyl sulfopalmitate |
| CN108889236B (en) * | 2018-07-27 | 2024-02-23 | 赞宇科技集团股份有限公司 | Drying and forming process and device for fatty acid methyl ester sodium sulfonate |
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| EP0506184A1 (en) * | 1991-03-28 | 1992-09-30 | Unilever N.V. | Detergent compositions and process for preparing them |
| CN1087945A (en) * | 1992-09-30 | 1994-06-15 | 亨克尔两合股份公司 | The preparation method of partical surface active agent |
| CN102277238A (en) * | 2011-07-13 | 2011-12-14 | 杭州迪康生物技术有限公司 | Granular fatty acid methyl ester sulfonate (MES)-containing composite |
| CN103320235A (en) * | 2013-06-21 | 2013-09-25 | 纳爱斯集团有限公司 | Particles containing sodium fatty acid methyl ester sulfonate and preparation method thereof |
| CN203807433U (en) * | 2014-02-12 | 2014-09-03 | 浙江赞宇科技股份有限公司 | Continuous preparation device for powdery MES particles |
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| EP0506184A1 (en) * | 1991-03-28 | 1992-09-30 | Unilever N.V. | Detergent compositions and process for preparing them |
| CN1087945A (en) * | 1992-09-30 | 1994-06-15 | 亨克尔两合股份公司 | The preparation method of partical surface active agent |
| CN102277238A (en) * | 2011-07-13 | 2011-12-14 | 杭州迪康生物技术有限公司 | Granular fatty acid methyl ester sulfonate (MES)-containing composite |
| CN103320235A (en) * | 2013-06-21 | 2013-09-25 | 纳爱斯集团有限公司 | Particles containing sodium fatty acid methyl ester sulfonate and preparation method thereof |
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